Method of producing methyl alcohol from waste products of the caustic-soda-cellulose process.



H. 0. V. BERGSTROM & 0. FAGERLIND. x. u. PAGHRLIND (wIDow) AND n. n. Ammann lemnnmm, nnrnnsmrmnvns or o. PAGEBLIND, nno'D.

METHOD 0F PRODUOING METHYL ALCOHOL FROM WASTE PRODUCTS 0F THE OAUSTIG SODA UELLULOSB PROCESS.

1,032,982. APPLICATION FILED JULY 13, 190B. 16

- To all whom t may concern:

, STATES PATENT OFFICE.; f

HILDING OLOE vnmn BEEGsTEM, OE sTOcKHOLM, SWEDEN, AND 'OSCAR EAGEELIND,

DECEASED; KERSTIN MARIA EAGERLIND, (WIDOW,) AND ERIK HJALMAE BERTILfA ALMGEEN, (CUAED1AN,) EEPEESENTATIvEs OF THE v ESTATE OE SAID OSCAR FAGERLIND, DEQEASED.

METHOD or PEODUCING'METHYL ALCOHOL FROM WASTE PRODUCTS or THECAUSTIC- SODA-'CELLULOSE PROCESS.

speeifieetien ef Letters Patent. 'Application mea July 1s, 1909. serial 110.5073415.

Patented July 1 6; 1912.

Beit known that I, HILDINC OLOEVIDAR BERCsTRM, a subject of the King of Sweden, and resident of Norrtullsgatan 29, Stockholm, Sweden, and the deceased OSCAR lEAGimLIND,Av late a subject of the King of Sweden, have invented certain new and'useful Improvements in the Method of Producing Methyl Alcohol from Waste Products of the Caustic-Soda-Cellulose Process,of which the following is a specification.

In manufacturing cellulose by boiling wood with a lye the principal constituent of which is caustic soda, vapors are given olf from the boiling 'lye, either when the pressure in the boiler Jis reduced during the boiling operation, or when the boiling lye is afterward evaporated. In some factories these vapors are condensed in surface condensers whereby a liquid of condensation is obtained( which princlpally consists of water `where this is permissible.

'with' sometimes an oil flowing on the surface of the same. In other factories these vapors are discharged into the atmospheric air. The water above referred Ato which contains bad-smelling products is generally discharged as water into .a river or the like Now, we have found. that the above mentioned liquid of condensation contains valuable products in such great quantities that the extraction of the same can be made of advantage. The most valuable` of these products is the methyl alcohol which can be obtained in a ve'ry pure state'. Among other products present in the said liquid sulfureted hydrogen, mercaptans, organic sulds, acetone,l

ammonia, amins may be mentioned, some of these products are, however, to be regarded as impurltles. -Such of the above mentloned products as contain sulfur are, of course,

only' obtained in factories where the so called sulfate method is employed and where the loss bf alkali is compensated for by adding sodium sulfate to the lye, but

. not in factories where the so-oalled, soda process is used and where the loss of alkali is compensated for in any other wayfor 1nstance by adding sodiumcarbonate to the lye. y l The present invention consists in that the said liquid of condensation forming at presi ent an'inconvenient waste product is treated for recoveringmethyl alcohol (wood spirit) from the same by a process to be more particularly explained hereinafter and A which is principally characterized b fact that theliquid vof condensation 1S exposed to fractional distillation and that'the fractions are treated with chemicals, if necessary, and further distilled. The water remaining after the completion of the process is practically pure and .may be discharged into a river or be employed Within the fac' tory. In the fractional distillation the orthe ganic sulfurous compounds are recovered as separate fractions. Ammoniaand sulfureted 'hydrogen combine to form Suld of ammonium and the methyl alcohol isv ob-v tained" as a separate more or less pure fraction. This fraction is or may be cleaned by a systematic treatment with suitable chemicals, such as acids, bases, oxidizing agents, metal salts, etc. After this treatmentv the solution may be exposed to fractional d istillation and rectification. The liquid may of course be treated with alkalis directly before being exposed to fractionalpdistillation. A .i

In order to make the process as economical as possible according to the present iny vention the heat of the vapors given off` from the boiling lye during the process is obtained by condensation and utilizedas a source of heat for conducting the distillation. This distillation may be performed in 4a column or other similar device, andthe heating effect of the vapors may be applied either directly or indirectly, z'. e., the vapors may be driven directly through the liquid of condensation, which is to be distilled, whereby fthe volatile constitutents of the same are driven of with the said vapors, or the vapors may be led through heating coils or elements placed inthe said liquid, whereby the vapors are condensed thereby gi'vlng olf their heat to the surrounding liquid which is brought to the boiling temperature.

In orderl that the invention may be' the Y better understood reference will be had to the accompanying drawings whereinw Figure 1 is a diagrammatic view of an ico apparatus. yemployed in conjunction with the process; and Fig. 2 is a view similar to Fig.

. l, illustrating a further form of apparatus.

Below we have indicated a practical method of carrying out the present invention, reference being had to Fig. l of the accompanying drawing.4 The vapors escaping from the boiling lye contained in the boiler A are led through a condenser B in which one part of the vapors of the less volatile constituents are condensed by the cooling action of water led around the serpentine E. llhe liquid of condensation thereby formed is allowed to descend `into the receptacle C where the same is penetrated by and subjected to the heating action of that part of the vapors which fhas not been condensed in the condenser B and which carrywith them the more'volatile constituents of the contents of the receptacle C. rlhe vapors escaping from the receptacle C are finally condensed in the refrigerator D by the action of cooling water led around theserpentine F. In said refrigerator a more or less concentrated solution containing methyl alcohol is obtained, the degree of concentration of which depends on the quantity of methyl alcohol vapors concentrated in the receptacle C. The solution inclosed in the receptacle C is tapped off and may be' distilled for the recovery of the small quantities of methyl alcohol contained in the same. lThe liquid coming from the refrigerator D, and liquid obtained by cooling directly the vapors escaping from the boiling lye, forms the raw-material, in the manufacture of methyl alcohol according to the present invention.

' This solution is thenintroduced most suitably into a continually working column where vit is concentrated further up to about 10-50% of alcohol. From this device a solution containing alcohol and having sometimes an oil floating thereon is obtained; this oil contains small quantities of methyl alcohol and is washed with water for removing the` said alcohol, and then the Washing water is miXed with the alcohol solution which is now distilled, for instance, in a periodically working column. The fraction containing the methyl alcohol is then, if necessary, treated with sulfuric acid for removing ammonia, and the sulfuric acid having been removed the said fraction may be treated with lead-acetate for removing mercaptans, and. sulfureted hydrogen. These substances may of course be separated from the methyl alcohol by distillation. Instead of lead-acetate other heavy metallic salts which cause a precipitate with sulfureted hydrogen can also be used. lf desired,

.the solution may then be treated' with hyr before being exposed to fractional distil.

lation.

incassa ln the form of apparatus shown in Fig.

led by tube ll through the coil Gr placed in a receptacle l filled with liquid of condensation, whereby said vapors are partly condensed. rllie liquid of condensation and the vapors not condensed in the coil G are led`through `the coil K surrounded by cooling water in the receptacle L whereby said vapors are condensed. rllhe liquid of condensation flows into the receptacle M from which it is, by means of a pump N or the like, carried over through tube O into the receptacle l. 'lhc`liquid in t-his .receptacle is heated to boiling temperature by the vapors passing through the coil G, and the vapors thereby escaping from said liquid are conilensed by being led through the coil R surrounded by cooling water in the receptacle l?.

Having no-w described our invention, what we claim as new, and desire to secure by lietters Patent is:

l. The herein described method of producing methyl alcohol from waste products of the soda cellulose process, which consists in condensing thevapors formed in the boiler during certain stages of the process, fractionally distilling the liquid of condensation formed thereby, and treating the fractions containing methyl alcohol with chemicals adapted to remove the impurities, substantially as described.

2. The herein described method of producing methyl alcohol from waste products ofthe soda cellulose process, which consists in condensing the vapors formed in the Yboiler during certain stages of the process, fractionally distilling the liquid of condensation formed thereby by means of the vapors coming from the said boiler, .and treating the fractions containing methyl alcohol with chemicals adapted to remove the impurities, substantially as described. l

3. The herein described method of producing alcohol from waste products of the soda cellulose process, which consists in condensing the vapors formed in the boiler during certain stages of the process, treating the liquid of condensation with chemica s adapted to removethe impurities, fractionally di'stilling the said liquid of condensation and recovering the fraction containing methyl alcohol, substantially as dcscribed.

4.'The herein described method of producing methyl alcohol (wood spirit) from Waste products of the caustic soda cellulose process, which consists in condensing vapors escaping from the liquid boiling lye, and distilling the liquid of condensation formed thereby, and recovering the fraciso ducing methyl alcohol-(Wood spirit) from Waste products of the caustic soda cellulose process, which consists in condensing vapors escaping from the .liquid boiling lye, distilling the liquid of condensation formed thereby, recovering the fraction or fractions containing methyl alcohol, and treating said fraction or fractions with chemicals adapted to remove impurities, substantially as described.

ducing methyl alcohol (Wood spirit) from waste products of the caustic soda cellulose `iufocess,`wh1ch consists 1n condensing vapors escaping from vthe liquid boiling lye, treat-'" ing the liquid of condensation formed thereby with chemicals adapted to remove the impurities, distilling the said liquid of condensation,l and recovering the fraction' or fractions'. containing methyl alcohol, substantially as described.

8. The herein described method of ,producing methyl alcohol (Wood spirit) from `.vaste products of the caustic soda cellulose process, which consists in condensing'vapors escaping from thev liquid boiling lye, treating the liquid of condensation formed therebywith vchemicals adapted to remove the impurities, distilling the said liquid of condensation, V recovering the fraction or fractions containing methyl alcohol and treating the said fraction or fractions with chemicals adapted' to remove the impurities, .substantially as described.

9. The herein described method of producing methyl alcohol (Wood spirit) from Waste products of the caustic soda cellulose process, Which consists incondensing vapors escaping from the liquid boiling lye treating the liquid of condensationwith chemicals adapted to remove the impurities, distilling the said liquid of condensation,-

recoyering the fraction or fractions containing methyl alcohol, treating the said fraction or fractions With chemicals adapted to remove the impurities and distilling the liquid thus treated, substantially as described.

10. The 'herein described method of producing methyl alcohol (Wood spirit) from Waste products of the caustic soda cellulose process, which consists in condensing the 'vapors escaping from the liquid boiling lye, distilling the liquidv of condensation formed thereby by means of vapors from the liquid boiling lye, and recovering the Ifraction or fractions containing methyl alcohol,v sub stant-ially as described.

In witness whereof, We have hereunto signed our names in t-he subscribing witnesses.

. HILDING OLOF VIDAR BERGSTRM. KERSTIN MARIA FAGERLIND, i ERIK HJLMAR BERTIL LMGREN,

Representatives of Oscar FagerZ'ind,-deceased.

Witnesses f ToRvALD NYsTRM, AXEL EHRNERF.

presence of two 

